1-Chloro-4-(chloromethyl)benzene → HCID 178509292、化合物

HRID 259085

反応式

HRID 259085 の反応式
[NH2:1][C:2]1[N:6]=[C:5]([SH:7])[NH:4][N:3]=1.[Cl:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13]Cl)=[CH:11][CH:10]=1>[OH-].[Na+].C(O)C>[NH2:1][C:2]1[N:6]=[C:5]([S:7][CH2:13][C:12]2[CH:15]=[CH:16][C:9]([Cl:8])=[CH:10][CH:11]=2)[NH:4][N:3]=1

参加物

5

反応物 2

HCID 77231-Chloro-4-(chloromethyl)benzeneHCID 1785092965-amino-1H-1,2,4-triazole-3-thiol2 回

生成物 1

HCID 178509292HCID 178509292、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A mixture of 3-amino-5-mercapto-s-triazole (Compound 5) [4.64g; 40 mmoles] in 40 ml. of IN sodium hydroxide was stirred at room temperature while solution of p-chlorobenzylchloride [7.55g; 48 mmoles] in 80 ml of absolute ethanol was added. The mixture was then warmed to 70°-75° and stirred for 30 minutes. The amber colored solution was then evaporated to 40 ml at reduced pressure, diluted with 50 ml of water and chilled overnight. The crude product was separated by filtration, air dried, and recrystallized two times from chloroform to afford 4.3g (45%) of analytically pure product that had a melting point of 107°-8°.

後処理

  1. additionwas added
  2. temperatureThe mixture was then warmed to 70°-75°
  3. customThe amber colored solution was then evaporated to 40 ml at reduced pressure
  4. additiondiluted with 50 ml of water
  5. temperaturechilled overnight
  6. customThe crude product was separated by filtration, air
  7. customdried
  8. customrecrystallized two times from chloroform
  9. customto afford 4.3g (45%) of analytically pure product that

出典と根拠

ORDレコード
ord-eb3a8c657c95425085bb668a31f5529f
出典データセット
uspto-grants-1977_07
特許番号
US04036840

関連ノート

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